CN1780738B - Fluid ejection device with compressive alpha-tantalum layer and manufacturing method thereof - Google Patents
Fluid ejection device with compressive alpha-tantalum layer and manufacturing method thereof Download PDFInfo
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- CN1780738B CN1780738B CN200480011680.1A CN200480011680A CN1780738B CN 1780738 B CN1780738 B CN 1780738B CN 200480011680 A CN200480011680 A CN 200480011680A CN 1780738 B CN1780738 B CN 1780738B
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- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 160
- 239000012530 fluid Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000000758 substrate Substances 0.000 claims abstract description 46
- 238000002161 passivation Methods 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 62
- 239000010936 titanium Substances 0.000 claims description 47
- 239000010955 niobium Substances 0.000 claims description 44
- 229910052758 niobium Inorganic materials 0.000 claims description 38
- 229910052782 aluminium Inorganic materials 0.000 claims description 37
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 37
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 36
- 229910052719 titanium Inorganic materials 0.000 claims description 36
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 35
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 30
- 239000004411 aluminium Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 23
- 230000008878 coupling Effects 0.000 claims description 20
- 238000010168 coupling process Methods 0.000 claims description 20
- 238000005859 coupling reaction Methods 0.000 claims description 20
- 230000008021 deposition Effects 0.000 claims description 20
- 239000010410 layer Substances 0.000 description 136
- 229910010271 silicon carbide Inorganic materials 0.000 description 35
- 230000006835 compression Effects 0.000 description 33
- 238000007906 compression Methods 0.000 description 33
- 235000012431 wafers Nutrition 0.000 description 31
- 239000000976 ink Substances 0.000 description 18
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 18
- 238000000151 deposition Methods 0.000 description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- 239000007789 gas Substances 0.000 description 16
- 229910052581 Si3N4 Inorganic materials 0.000 description 13
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 13
- 239000013078 crystal Substances 0.000 description 12
- 229910010293 ceramic material Inorganic materials 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 11
- 239000002390 adhesive tape Substances 0.000 description 8
- 229910052786 argon Inorganic materials 0.000 description 8
- 238000004544 sputter deposition Methods 0.000 description 8
- 229910018182 Al—Cu Inorganic materials 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 238000004062 sedimentation Methods 0.000 description 7
- 239000012528 membrane Substances 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 238000001755 magnetron sputter deposition Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000005137 deposition process Methods 0.000 description 4
- 238000010894 electron beam technology Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 238000000608 laser ablation Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 230000003628 erosive effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical class CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 230000003325 follicular Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000002821 niobium Chemical class 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2/00—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed
- B41J2/005—Typewriters or selective printing mechanisms characterised by the printing or marking process for which they are designed characterised by bringing liquid or particles selectively into contact with a printing material
- B41J2/01—Ink jet
- B41J2/135—Nozzles
- B41J2/14—Structure thereof only for on-demand ink jet heads
- B41J2/14016—Structure of bubble jet print heads
- B41J2/14088—Structure of heating means
- B41J2/14112—Resistive element
- B41J2/14129—Layer structure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41J—TYPEWRITERS; SELECTIVE PRINTING MECHANISMS, i.e. MECHANISMS PRINTING OTHERWISE THAN FROM A FORME; CORRECTION OF TYPOGRAPHICAL ERRORS
- B41J2202/00—Embodiments of or processes related to ink-jet or thermal heads
- B41J2202/01—Embodiments of or processes related to ink-jet heads
- B41J2202/03—Specific materials used
Abstract
A fluid ejection device (300) is disclosed. The fluid ejection device (300) may include a substrate (301) including a heating element (306) and a passivation layer (308, 310) in contact with the heating element (306). The fluid ejection device (300) may further include a buffer layer (312) in contact with the passivation layer (308, 310) and a compressive alpha-tantalum layer (314) in contact with, and lattice matched to, the buffer layer (312).
Description
Background technology
Tantalum (Ta) film is widely used in semiconductor and microelectromechanical systems (MEMS) manufacturing.For example, in semiconductor integrated circuit was made, tantalum can be as the diffusion impervious layer between copper and the silicon.Tantalum also can be used as the grid in mos field effect transistor (MOSFET) device.Tantalum can also be used for absorbing X ray at the X ray mask.For example in the printhead, tantalum is used as the top layer of resistor and other substrate layer, exempts from the infringement of the cavitation erosion that is caused by the collapse of China ink bubble to protect following layer in hot ink-jet microelectromechanical systems.Tantalum layer also can protect the layer below the printhead to exempt from and ink generation chemical reaction.
Metastable cubic phase tantalum is called β-phase or " β-tantalum ", is typically applied in the hot ink-jet apparatus manufacturing.This β-tantalum layer is a fragility, and it is unstable to become after temperature increases.After surpassing 300 ℃, β-tantalum is transformed into body-centered cubic (bcc) α-phase or " alpha-tantalum ".Alpha-tantalum is the body balance or the stable phase of tantalum.Expectation forms stable compression alpha-tantalum film on the fluid ejection apparatus.This compression alpha-tantalum film can be by the service life that stops peeling off on the substrate, blistering or layering to improve described device.
Summary of the invention
The present invention discloses a kind of fluid ejection apparatus.This fluid ejection apparatus can comprise the substrate that contains heating element heater and with the contacted passivation layer of heating element heater.Fluid ejection apparatus may further include contact with the contacted cushion of passivation layer with cushion and with the compressive alpha-tantalum layer of its lattice coupling.
Description of drawings
Following accompanying drawing shows in order to realize exemplary embodiment of the present invention.Identical Reference numeral is represented the same parts in different views in the accompanying drawing or the embodiment.
Fig. 1 is the flow chart that forms the method for compressive alpha-tantalum layer according to one embodiment of the present invention on substrate.
Fig. 2 is the cross-sectional illustration according to the compression alpha-tantalum film of one embodiment of the present invention.
Fig. 3 is the cross-sectional illustration that comprises the fluid ejection apparatus that compresses alpha-tantalum according to one embodiment of the present invention.
Fig. 4 is the corresponding X ray diffracting data figure that the compression alpha-tantalum film of titanium cushion is arranged according to the growth of one embodiment of the present invention.
Fig. 5 is the corresponding X ray diffracting data diagram that the compression alpha-tantalum film of niobium cushion is arranged according to the growth of one embodiment of the present invention.
Fig. 6 is the corresponding X ray diffracting data figure that the compression alpha-tantalum film of basic fine aluminium cushion is arranged according to the growth of one embodiment of the present invention.
Fig. 7 is the corresponding X ray diffracting data figure that the compression alpha-tantalum film of Al-zn-mg-cu alloy cushion is arranged according to the growth of one embodiment of the present invention.
The specific embodiment
The specific embodiment of the present invention is included in the method that forms compressive alpha-tantalum layer on the substrate.The present invention has also disclosed compression alpha-tantalum film, fluid ejection apparatus, hot ink-jet print head and thermal ink jet printers.Below with reference to the exemplary embodiment shown in the accompanying drawing, and will adopt specific term to describe them.But, it should be understood that scope of the present invention do not wish so be restricted.Here the change of shown creative feature and further revise and by it may occur to persons skilled in the art that based on the additional application of shown inventive principle here, and, should be considered as comprising within the scope of the present invention to the ownership of this disclosure.
Hot ink-jet (TIJ) printhead comprises silicon substrate typically, has conductive layer and resistive layer on it so that electrical property to be provided, and is used for heating and sprays ink from printhead.Resistive layer is used for heating ink to vaporization, forms bubble.The ink steam expansion forms bubble, and ink is ejected from printhead, on common targets such as paper, becomes a single point or pixel as ink droplet jet.Terminology used here " ink-jet " means the whole process that comprises heating ink, ejects the collapse of ink and ink steam bubble with ink droplets.
The problem relevant with traditional hot ink-jet print head be included in ink droplets with and subsequent process in the fault of corrosive nature generation of the mechanical shock (cavitation erosion) that produces of the high thermal-mechanical stress, black follicular rupture that cause and ink.Because these reasons are provided with the life-span that protective layer prolongs printhead usually on the resistance that forms printhead and other layer.
Resistive element on the print head substrate (being called heating element heater sometimes at this) is passivated layer for example silicon nitride (SiN) and/or carborundum (SiC) and for example tantalum covering of cavitation erosion barrier layer usually.Silicon nitride is ceramic material and electrical insulator, can avoid short circuit by protective resistor.Carborundum is hard semi-conducting material and impalpable structure.Carborundum is used to stop ink to infiltrate and arrives layer below the printhead, and mechanical strength is provided.Tantalum has good mechanical strength, can bear ink and spray the thermal-mechanical stress that causes.In addition, tantalum has chemical inertness when high temperature, can minimize the corrosion that ink causes.
Tantalum layer is usually by metastable cubic phase tantalum, and promptly β-phase or " β-tantalum " are formed.This β-tantalum layer is a fragility, and it is unstable to become after temperature increases.
Fig. 1 is the flow chart that forms the method 100 of compressive alpha-tantalum layer according to the embodiment of the present invention on substrate.Substrate can be formed by semi-conducting material.Substrate can comprise other material layer, comprises silicon nitride (SiN) material and/or carborundum (SiC) layer.Silicon carbide layer can be on substrate surface.Method 100 can be included in and deposit cushion 102 on the substrate and deposit compressive alpha-tantalum layer 104 on cushion, and lattice coupling between compressive alpha-tantalum layer and the cushion.The thickness range of compressive alpha-tantalum layer can be from about 10 dusts
To about 4 microns (μ m).
The lattice-site that term " lattice coupling " means on the material crystals face that forms mutual interface mates approximate geometrically mutually in its both sides, interface.For two different crystal faces are being mated geometrically in its both sides, interface, the symmetry that requires them almost is identical, and their lattice mismatches each other are less than about 5%.Be defined in the list of references that lattice coupling is also quoted in " Strained LayerSuperlattices; Semiconductors and Semimetals; Vol.33; R.K.Willardson and A.C.Beer (Academic, New York, 1990) write ", " J.A.Venables; G.Spiller; and M.Hanbucken, Rep.Prog.Phys:47,399 (1984) " and they.
Can adopt any suitable physical gas phase deposition technology to realize deposition 102 cushions and deposition 104 compression alpha-tantalums.For example, can adopt sputter, laser ablation, electron beam and hot evaporation coating technique separately, the technology that perhaps adopts them is in conjunction with depositing 102 and 104, and certainly, the present invention is not limit by above-mentioned technology.Deposition 102 and 104 can be finished comprising under underlayer temperature is less than any temperature of 300 ℃.And, deposit 102 cushions and may further include the use substrate bias.When using traditional direct current magnetron sputtering system, the bias voltage scope from about 0 volt to approximately-500 volt.
Deposit 102 cushions and can comprise the deposition titanium layer.The thickness of titanium layer can be from about 3 monoatomic layers to approximately according to the embodiment of the present invention
The present preferred thickness range of other embodiment titanium cushion according to the present invention can be at least from approximately
Beginning.According to the embodiment of the present invention, in order to obtain the smooth substrate surface of atom level, the thickness of expectation titanium layer is the same thin with a monoatomic layer.In one embodiment, the orientation of titanium layer on substrate can be that titanium crystal [100] direction is perpendicular to substrate.According to another embodiment, the lattice coupling can appear between titanium layer and the compressive alpha-tantalum layer.
Deposit 102 cushions and can comprise deposition niobium layer.The thickness of niobium layer can be from about 3 monoatomic layers to approximately according to the embodiment of the present invention
According to the embodiment of the present invention, in order to obtain the smooth substrate surface of atom level, the thickness of expectation niobium layer is the same thin with a monoatomic layer.The present preferred thickness range of other embodiment niobium cushion according to the present invention can be at least from approximately
Beginning.
In another embodiment, deposit 102 cushions and can comprise basic fine aluminium of deposition or Al-zn-mg-cu alloy layer.The copper that the Al-zn-mg-cu alloy layer comprises can reach about 10% weight ratio.The thickness range of basic fine aluminium or Al-zn-mg-cu alloy layer can be from about 3 monoatomic layers to approximately
Consistent with embodiments of the present invention.According to the embodiment of the present invention, in order to obtain the smooth substrate surface of atom level, expect that the thickness of basic fine aluminium or Al-zn-mg-cu alloy layer is the same thin with a monoatomic layer.
Fig. 2 is the cross-sectional illustration according to a compression alpha-tantalum pellicular cascade 200 of embodiment of the present invention.This compression alpha-tantalum pellicular cascade 200 can comprise with substrate 202 contacted ceramic materials 204, with ceramic material 204 contacted cushions 206 and with the compressive alpha-tantalum layer 208 of cushion 206 lattices couplings.Ceramic material 204 can comprise carborundum (SiC).Cushion can comprise at least a in titanium, niobium, basic fine aluminium and the Al-zn-mg-cu alloy.
Fig. 3 is the cross-sectional illustration that comprises the fluid ejection apparatus that compresses alpha-tantalum according to embodiment of the present invention.This fluid ejection apparatus 300 can comprise and corresponding to hot ink-jet print head of embodiment of the present invention or thermal ink jet printers.Fluid ejection apparatus 300 can comprise substrate stack 301.Substrate stack 301 can comprise resistive element 306, main substrate 302, optional cover layer 304, insulating ceramic materials 308 and ceramic material 310.Fluid ejection apparatus 300 may further include cushion 312 that is formed on second ceramic material 310 and the compressive alpha-tantalum layer 314 that mates with cushion 312 lattices.
Cover layer 304 can comprise for example thermal oxide layer, silica (SiO
2) layer or tetraethyl orthosilicate salt (TEOS) layer, the present invention is not limit by above-mentioned example certainly.Cushion 312 contacts with second ceramic material 310.Similarly, cushion 312 contacts with compression alpha-tantalum 314.Insulating ceramic materials 308 can comprise silicon nitride (SiN).Second ceramic material 310 can comprise carborundum (SiC).Can adopt at least a following physical gas phase deposition technology on second ceramic material 310, to form cushion 312: sputter, laser ablation, electron beam and hot evaporation.The thickness range of compressive alpha-tantalum layer 314 can be from approximately
To about 4 μ m.According to the embodiment of the present invention, cushion 312 can be formed by the material that for example lattice coupling forces tantalum to grow up to the alpha-tantalum squeezed state by any.In some embodiments, cushion is one of them of titanium, niobium, basic fine aluminium and Al-zn-mg-cu alloy at least, is further explained below with reference to embodiment.
Embodiment 1: the titanium cushion
In this embodiment, cushion 312 can be formed by titanium layer.Can be according to the thickness range of this titanium layer of embodiments of the invention from about 3 monoatomic layers to approximately
Just as mentioned above, can be at least from approximately according to the present preferred thickness range of other embodiments of the invention titanium cushion
Beginning.The crystal structure of titanium is close-packed hexagonal structure (hcp).In one embodiment of the invention, the orientation of titanium layer on substrate stack 301 can be that titanium crystal [100] direction is perpendicular to substrate stack 301.In another embodiment, titanium layer can include the titanium crystal grain of texture.
The tectal orientation of tantalum is Ta[110] direction is perpendicular to the substrate that compressive residual stress is arranged.Lattice coupling between the Ti/Ta interface is forced tantalum cover layer growth body-centered cubic (bcc) alpha-tantalum phase.
The method that following table 1 shows according to the embodiment of the invention has the parameter that obtains titanium cushion and the tectal test wafers 1-5 of compression alpha-tantalum from five.Every wafer comprises the main silicon substrate with silicon nitride and silicon carbide passivation layer.For each piece wafer, at first sputtering sedimentation titanium cushion, sputter compressive alpha-tantalum layer then on silicon carbide.The 2-3 of table 1 row show with
The thickness of the tantalum/titanium that calculates (Ta/Ti) layer and the alpha-tantalum membrane stress that calculates with Megapascal (MPa).Row 4-5 shows the deposition parameter of each tantalum layer, promptly with SCCM (calibrating gas flow velocity under atmospheric pressure is 1 standard cubic centimeter per minute) argon gas flow velocity that calculates and the ar pressure that calculates with millitorr (mTorr).Row 6 show the plasma power that uses in the sputter deposition process that calculates with thousand-watt (kW).Thinner titanium layer plasma power is reduced to 1.5kW from 3kW, to increase the accuracy of THICKNESS CONTROL.Titanium layer is grown under the condition of ar pressure 2.5mTorr and argon gas flow velocity 100SCCM.Certainly, those skilled in the art should know that above-mentioned plasma power scope, ar pressure and the flow velocity that sets for specific embodiment is as exemplary setting, and other scope of these parameters and setting are also within the scope of the invention.
Table 1
Comprise the titanium cushion the embodiment of the invention be in the alpha-tantalum film that forms, inside or residual stress to be arranged on the other hand.Following substrate layer, for example silicon nitride (SiN) and carborundum (SiC) are bearing compression stress.Because this additional reason, this alpha-tantalum cover layer is grown in compression to avoid blistering and layering substantially.
In this embodiment, the alpha-tantalum film in the table 1 is grown under compression stress.In deposition process, do not apply bias voltage on the substrate.Certainly, in some embodiments, on substrate, apply bias voltage if necessary the alpha-tantalum film is more compressed.According to the embodiment of the present invention, tantalum and titanium layer use the direct current magnetron sputter deposition.Certainly,, also can use other physical gas phase deposition technology according to other embodiments of the invention, for example laser ablation, electron beam and hot evaporation coating technique, and the present invention is not limit by above-mentioned technology.
Adopt Scotch
TMThe adhesive tape method has been measured the adhesion strength of Ta/Ti bilayer with silicon carbide passivation layer.Attempt to adopt Scotch
TMAdhesive tape is peeled off silicon carbide passivation layer with the Ta/Ti bilayer.The Ta/Ti bilayer fails to peel off.In one embodiment, the secure adhesion between Ta/Ti bilayer and the silicon carbide passivation layer can form titanium carbide (TiC) covalent bond between the SiC/Ti interface, and the strong bonding between the SiC/Ti boundary layer is provided.In addition, the key between compression alpha-tantalum top layer and its titanium cushion is a key.
Fig. 4 grows on test wafers 2 according to the method 100 of embodiment of the present invention the corresponding X ray diffracting data figure of the compression alpha-tantalum of titanium cushion film is arranged.Among Fig. 4, the angle of diffraction that the representative of x-axle is calculated with angle, the intensity that the representative of y-axle is calculated with arbitrary unit.The compression alpha-tantalum is deposited on
On the thick titanium layer.The diffraction cutting edge of a knife or a sword is corresponding with the alpha-tantalum of [110] orientation.Show drawn on the figure that embeds in order to explain the vertical line of desired β-Ta (002) and α-Ta (200) reflection peak position.These desired reflections do not exist, and show α-Ta (110) layer of the good orientation of having grown on test wafers 2.Because the overlap of peaks of α-Ta (110) and its Ti (100) cushion so the reflection peak of Ti has been covered, does not therefore occur in Fig. 4.In addition, the diffracted ray number of X-ray scanning shown in Figure 4 has disclosed the list-phase α-Ta cover layer of [110] orientation, show on the diffraction maximum small asymmetric may be owing to the titanium cushion of unreacted [001] texture.
Following table 2 shows the X-ray diffraction data of the test wafers 1-5 in the table 1.The row 2-6 unit of showing is
Thickness, tantalum phase, the unit of tantalum/titanium (Ti/Ta) layer be
Alpha-tantalum spacing of lattice, unit be
The tantalum crystallite dimension and the rocking curve of half peak overall with (FWHM) of the alpha-tantalum that calculates with angle.The width of rocking curve provides the distribution of orientations of the cylindric crystal grain of alpha-tantalum that calculates with angle.Tantalum crystallite dimension and rocking curve data show that thickness is
With
The titanium cushion desirable bigger tantalum crystallite dimension is provided, promptly approximate 130 dusts and narrower grain orientation distribute.
Table 2
Embodiment 2: the niobium cushion
In this embodiment, cushion 312 can be formed by the niobium layer.Can be according to the thickness range of this niobium layer of other embodiment of the present invention from about 3 monoatomic layers to approximately
Just as mentioned above, the present preferred thickness range of other embodiment niobium cushion according to the present invention can be at least from approximately
Beginning.Niobium and titanium are the member of same row in the periodic table of elements, have similar physical property.The crystal structure of niobium is body-centered cubic structure (bcc), and is identical with alpha-tantalum.Because the spacing of lattice of alpha-tantalum and niobium much at one, promptly be respectively
With
So tantalum (110) cover layer and niobium (110) face be the lattice coupling almost completely.Certainly different with tantalum, niobium can not grow up to beta phase structure.The foreign gas or the backing material type that exist on the irrelevant substrate, niobium grows up to the α phase structure usually.Because this character, when the niobium thin layer at first is deposited on the substrate stack 301, tantalum/niobium lattice coupling at the interface will force the tantalum cover layer to grow up to the alpha-tantalum phase.
Following table 3 shows according to embodiments of the invention has the parameter that obtains niobium cushion and the tectal test wafers 6-11 of compression alpha-tantalum from 6.Each piece wafer comprises the main silicon substrate with silicon nitride and silicon carbide passivation layer.For each piece wafer, at first sputtering sedimentation niobium cushion, sputter compressive alpha-tantalum layer then on silicon carbide.The niobium layer thickness variation of test wafers from
Arrive
The row 2-3 of table 3 show with
The thickness of the Ta/Nb layer that calculates and the alpha-tantalum membrane stress that calculates with MPa.Row 4-5 shows the deposition parameter of tantalum layer, just provides argon gas flow velocity that calculates with SCCM and the ar pressure that calculates with mTorr respectively.Row 6 show the plasma power that the difference sputtering sedimentation tantalum that calculates with kW and niobium layer use.According to another embodiment of the invention, plasma power is reduced to about 0.5kW can obtain thinner niobium layer so that more accurate THICKNESS CONTROL to be provided.According to an embodiment of the invention, the niobium cushion is grown under the condition of ar pressure 2.5mTorr and argon gas flow velocity 100SCCM.Certainly, those skilled in the art should know that above-mentioned plasma power scope, ar pressure and the flow velocity that sets for specific implementations is as exemplary setting, and other scope of these parameters and setting are also within the scope of the invention.
Table 3
Comprise the niobium cushion embodiment of the present invention be in the alpha-tantalum film that forms, inside or residual stress to be arranged on the other hand.Stress data shown in the table 3 shows that the alpha-tantalum film grows under compression stress.In addition, the thickness that shows with the niobium cushion of alpha-tantalum membrane stress has dependence.In deposition process, do not apply bias voltage on the substrate.According to other embodiment of the present invention, apply substrate bias and cause that the alpha-tantalum film more compresses.Tantalum and niobium layer use the direct current magnetron sputter deposition according to the embodiment of the present invention.Certainly,, also can use other physical gas phase deposition technology according to other embodiment of the present invention, for example laser ablation, electron beam and hot evaporation coating technique, and the present invention is not limit by above-mentioned technology.
Adopt Scotch
TMThe adhesive tape method has been measured the adhesion strength of Ta/Nb bilayer and silicon carbide passivation layer.Attempt to adopt Scotch
TMAdhesive tape is peeled off silicon carbide passivation layer with the Ta/Nb bilayer.The Ta/Nb bilayer fails to peel off.In one embodiment, adhesion strength can be owing to the metallicity bonding between tantalum and its niobium cushion.In another embodiment, niobium and alloying with silicon form the NbSi covalent bond at the interface at SiC/Nb, can guarantee the strong bonding between these layers.Reference example M.Zhanget al., Thin Solid Films, Vol.289, no.1-2, pp.180-83 and S.N.Songet al., Journal of Applied Physics, Vol.66, no.11, pp.5560-66.
Fig. 5 grows on test wafers 6 according to the method 100 of embodiment of the present invention the corresponding X ray diffracting data figure of the compression alpha-tantalum of niobium cushion film is arranged.Among Fig. 5, the angle of diffraction that the representative of x-axle is calculated with angle, the intensity that the representative of y-axle is calculated with arbitrary unit.The compression alpha-tantalum is deposited on
On the thick niobium layer.The diffraction cutting edge of a knife or a sword is corresponding with the alpha-tantalum of [110] orientation.Show drawn on the figure that embeds in order to explain the vertical line of desired β-Ta (002) reflection peak position.In addition, the arrow shown in the master map has shown the position of desired α-Ta (200) reflection peak.These desired reflections do not exist, and show α-Ta (110) layer of the good orientation of having grown on test wafers 6.Among Fig. 5, because the overlap of peaks of α-Ta (110) and its Nb (110) cushion, so desired niobium reflection peak has been covered.
Following table 4 shows the X-ray diffraction data of the test wafers 6-11 in the table 1.The row 2-6 unit of showing is
Thickness, tantalum phase, the unit of tantalum/niobium layer be
Alpha-tantalum spacing of lattice, unit be
The tantalum crystallite dimension and the rocking curve of the alpha-tantalum half peak overall with (FWHM) calculated with angle.Tantalum crystallite dimension shown in the table 4 and rocking curve data show that thickness is
The niobium cushion with respect to test wafers 6-10, provide to have that narrower grain orientation distributes and the bigger tantalum crystallite dimension of littler internal stress, but also reference table 3.
Table 4
Embodiment 3: basic fine aluminium cushion
In this embodiment, cushion 312 can be formed by basic aluminum layer.This cushion also can form alloy with copper, shown in the following examples 4.The crystal structure of aluminium is face-centred cubic structure (fcc), and Al (111) face and Ta (110) face lattice coupling.Because this character, when basic thin layer of pure aluminiurn at first is deposited on the substrate stack 301, tantalum/basic fine aluminium (Ta/Al) lattice coupling at the interface will be forced tantalum cover layer growth alpha-tantalum phase.
Following table 5 shows according to the embodiment of the present invention has the parameter that obtains basic fine aluminium cushion and the tectal test wafers 12-16 of compression alpha-tantalum from five.Each piece of wafer 12-16 all comprises the main silicon substrate with silicon nitride and silicon carbide passivation layer.For each piece wafer, the at first basic fine aluminium cushion of sputtering sedimentation, sputter compressive alpha-tantalum layer then on silicon carbide.According to the embodiment of the present invention, the basic fine aluminium buffer layer thickness of test wafers 12-16 change from
Arrive
The row 2-3 of table 5 show with
The thickness of the Ta/Al layer that calculates and the alpha-tantalum membrane stress that calculates with MPa.Row 4-5 shows the deposition parameter of tantalum layer, just provides argon gas flow velocity that calculates with SCCM and the ar pressure that calculates with mTorr respectively.Row 6 show the plasma power that the difference sputtering sedimentation tantalum that calculates with kW and basic aluminum layer use.According to the embodiment of the present invention, the fine aluminium cushion is grown under the condition of ar pressure 2.5mTorr and argon gas flow velocity 50SCCM substantially.Certainly, those skilled in the art should know that above-mentioned plasma power scope, ar pressure and the flow velocity that sets for specific implementations is as exemplary setting, and other scope of these parameters and setting are also within the scope of the invention.
Table 5
Comprise basic fine aluminium cushion embodiment of the present invention be in the alpha-tantalum film that forms, inside or residual stress to be arranged on the other hand.Stress data shown in the table 5 (row 3) shows that the alpha-tantalum film grows under compression stress.The compression stress that is grown in the alpha-tantalum on the basic fine aluminium cushion can be owing to basic fine aluminium cushion.Because tantalum/basic fine aluminium lattice coupling at the interface, the alpha-tantalum cover layer is forced to grow under compression stress.In addition, the alpha-tantalum membrane stress shows and the thickness of basic fine aluminium cushion has dependence.In deposition process, do not apply bias voltage on the substrate.According to other embodiment of the present invention, apply substrate bias and cause that the alpha-tantalum film more compresses.Tantalum and basic aluminum layer use the direct current magnetron sputter deposition according to the embodiment of the present invention.Certainly, according to other embodiment of the present invention, also can use other physical gas phase deposition technology.
Adopt Scotch
TMThe adhesive tape method has been measured the adhesion strength of Ta/Al bilayer with silicon carbide passivation layer.Attempt to adopt Scotch
TMAdhesive tape is peeled off silicon carbide passivation layer with the Ta/Al bilayer.The Ta/Al bilayer fails to peel off.In one embodiment, the bonding that adhesion strength can form at the interface owing to the metallicity bonding between tantalum and its aluminium cushion and SiC/Al has been guaranteed the strong adhesion between these layers.
Fig. 6 is according to grow on the test wafers 14 corresponding X ray diffracting data figure of compression alpha-tantalum film with basic fine aluminium cushion of the method 100 of embodiment of the present invention.Among Fig. 6, the angle of diffraction that the representative of x-axle is calculated with angle, the intensity that the representative of y-axle is calculated with arbitrary unit.Compressive alpha-tantalum layer is deposited on
On the thick basic aluminum layer.The diffraction cutting edge of a knife or a sword is corresponding with the alpha-tantalum of [110] orientation.Show drawn on the figure that embeds in order to explain the vertical line of desired β-Ta (002) reflection peak position.In addition, the arrow shown in the master map has shown the position of desired α-Ta (200) reflection peak.These desired reflections do not exist or are very little, show α-Ta (110) layer of the good orientation of having grown on test wafers 18.Because the overlap of peaks of α-Ta (110) and its Al (111) cushion, so desired Al (111) reflection has been covered.
Following table 6 shows the X-ray diffraction data of the test wafers 12-16 in the table 1.The row 2-6 unit of showing is
Thickness, tantalum phase, the unit of tantalum/basic aluminum layer be
Alpha-tantalum spacing of lattice, unit be
The tantalum crystallite dimension and the alpha-tantalum half peak overall with (FWHM) calculated with angle broadcast the pendulum curve.Tantalum crystallite dimension shown in the table 6 and rocking curve data show that thickness is
Basic fine aluminium cushion with respect to other test wafers, provide narrower grain orientation to distribute, shown in the reference table 5 with littler internal stress.
Table 6
Embodiment 4: the Al-zn-mg-cu alloy cushion
In this embodiment, cushion 312 can be formed by the Al-zn-mg-cu alloy layer.The copper that this Al-zn-mg-cu alloy cushion comprises can reach about 10 weight %, and all the other are basic fine aluminium.Because Solder for Al-Cu Joint Welding is more insensitive to the fault that electromigration causes, so Al-zn-mg-cu alloy is employed than basic fine aluminium is more frequent in integrated circuit (IC) industry.In addition, the basic fine aluminium rake thin that is used for sputter than Solder for Al-Cu Joint Welding rake thin more expensive and rareer arriving.As mentioned before, the crystal structure of aluminium is face-centered cubic (fcc), and Al (111) face and Ta (110) face lattice coupling.Because this character, when the Al-zn-mg-cu alloy thin layer at first is deposited on the substrate stack 301, tantalum/Al-zn-mg-cu alloy lattice coupling at the interface will be forced tantalum cover layer growth alpha-tantalum phase.In addition, the crystal structure of copper is face-centred cubic structure (fcc), and the copper foreign atom in the aluminium lattice can occupy the face-centered cubic position or replace the locational Al atom of face-centered cubic.
The method 100 that following table 7 shows according to embodiment of the present invention has the parameter that obtains Al-zn-mg-cu alloy cushion and the tectal test wafers 17-22 of compression alpha-tantalum from six.Be used for the copper that the Al-zn-mg-cu alloy rake thin of test wafers 17-22 comprises and can reach about 5 weight %, all the other are basic fine aluminium.Each piece wafer all comprises the main silicon substrate with silicon nitride and silicon carbide passivation layer.For each piece wafer, at first sputtering sedimentation Al-zn-mg-cu alloy cushion, sputter compressive alpha-tantalum layer then on silicon carbide.According to the embodiment of the present invention, the Al-zn-mg-cu alloy layer thickness variation of test wafers 17-22 from
Arrive
The row 2-3 of table 7 show with
The thickness of the Ta/Al-Cu layer that calculates and the alpha-tantalum membrane stress that calculates with MPa.Row 4-5 shows the deposition parameter of tantalum layer, just provides argon gas flow velocity that calculates with SCCM and the ar pressure that calculates with mTorr respectively.Row 6 show the plasma power that the difference sputtering sedimentation tantalum that calculates with kW and Al-zn-mg-cu alloy layer use.According to the embodiment of the present invention, the Al-zn-mg-cu alloy cushion is grown under the condition of ar pressure 5mTorr and argon gas flow velocity 100SCCM.Certainly, those skilled in the art should know that above-mentioned plasma power scope, ar pressure and the flow velocity that sets for specific implementations is as exemplary setting, and other scope of these parameters and setting are also within the scope of the invention.
Table 7
Comprise the Al-zn-mg-cu alloy cushion embodiment of the present invention be in the alpha-tantalum film that forms, inside or residual stress to be arranged on the other hand.Stress data shown in the table 7 (row 3) shows that the alpha-tantalum film grows under compression stress.The compression stress that is grown in the alpha-tantalum on the Al-zn-mg-cu alloy cushion can be owing to the Al-zn-mg-cu alloy cushion.Because tantalum/Al-zn-mg-cu alloy lattice coupling at the interface, the alpha-tantalum cover layer is forced to grow under compression stress.In deposition process, do not apply bias voltage on the substrate.According to other embodiment of the present invention, apply substrate bias and cause that the alpha-tantalum film more compresses.Tantalum and Al-zn-mg-cu alloy layer use the direct current magnetron sputter deposition according to the embodiment of the present invention.Certainly, according to other embodiment of the present invention, also can use other physical gas phase deposition technology.
Adopt Scotch
TMThe adhesive tape method has been measured the adhesion strength of Ta/Al-Cu bilayer with silicon carbide passivation layer.Attempt to adopt Scotch
TMAdhesive tape is peeled off silicon carbide passivation layer with the Ta/Al-Cu bilayer.The Ta/Al-Cu bilayer fails to peel off.In one embodiment, adhesion strength can owing between tantalum and its aluminium cushion and at SiC/Al-Cu metallic bond at the interface, guaranteed the strong combination between these layers.
Fig. 7 is according to grow on the test wafers 18 corresponding X ray diffracting data figure of compression alpha-tantalum film of Al-zn-mg-cu alloy cushion of the method 100 of embodiment of the present invention.Among Fig. 7, the angle of diffraction that the representative of x-axle is calculated with angle, the intensity that the representative of y-axle is calculated with arbitrary unit.Compressive alpha-tantalum layer is deposited on
On the thick Al-zn-mg-cu alloy layer.Peak in the master map is corresponding with the alpha-tantalum of [110] orientation.Show drawn on the figure that embeds in order to indicate the vertical line of desired Al (200) reflection peak position.In addition, the arrow shown in the master map has shown the position of desired α-Ta (200) reflection peak.These desired reflections do not exist or are very little, show α-Ta (110) layer of the good orientation of having grown on test wafers 18.Because the overlap of peaks of α-Ta (110) and its Al (111) cushion, so desired Al (111) reflection has been covered.
Following table 8 shows the X-ray diffraction data of the test wafers 17-22 in the table 7.The row 2-6 unit of showing is
Thickness, tantalum phase, the unit of tantalum/Al-zn-mg-cu alloy layer be
Alpha-tantalum spacing of lattice, unit be
The tantalum crystallite dimension and the rocking curve of the alpha-tantalum half peak overall with (FWHM) calculated with angle.As shown in table 8, the tantalum films on the wafer 17-22 has shown the crystal grain that disperses or extensively distribute.
Table 8
Should be appreciated that be used to the to explain application of specific embodiment of the invention principle of above-cited device and embodiment.Under the prerequisite that does not deviate from the spirit and scope of the invention, can design the device of revising and selecting on various forms and the details.Although the specific embodiment of the present invention has shown in the drawings and has been described with reference to aforesaid exemplary embodiment of the invention, but to those skilled in the art, obviously can make the modification on various forms and the details, and not break away from notion and the principle that limits in the claim of enclosing.
Claims (10)
1. fluid ejection apparatus comprises:
The substrate that comprises heating element heater;
With the contacted passivation layer of heating element heater;
With the contacted cushion of passivation layer; With
Contact with cushion and with the compressive alpha-tantalum layer of its lattice coupling.
2. fluid ejection apparatus according to claim 1, cushion wherein comprises titanium layer.
3. fluid ejection apparatus according to claim 1, cushion wherein comprises the niobium layer.
4. fluid ejection apparatus according to claim 1, cushion wherein comprises basic aluminum layer.
5. fluid ejection apparatus according to claim 1, cushion wherein comprises the Al-zn-mg-cu alloy layer.
6. the manufacture method of a fluid ejection apparatus comprises:
On substrate, form heating element heater;
On heating element heater, deposit cushion; With
At the buffer layer deposition compressive alpha-tantalum layer, lattice coupling between compressive alpha-tantalum layer and the cushion.
7. method according to claim 6, deposition cushion wherein comprise one of titanium deposition, niobium, basic fine aluminium and Al-zn-mg-cu alloy layer.
8. a fluid ejection apparatus comprises;
Be formed on the heating element heater on the substrate;
With the contacted passivation layer of heating element heater; With
A kind of coupling by lattice, force tantalum to grow into the means of compressive alpha-tantalum layer, and alpha-tantalum layer wherein is grown on the passivation layer.
9. fluid ejection apparatus according to claim 8, compulsive means wherein comprise buffer layer deposition on passivation layer, lattice coupling between compressive alpha-tantalum layer wherein and the cushion.
10. fluid ejection apparatus according to claim 9, cushion wherein comprise one of them of titanium, niobium, basic fine aluminium and Al-zn-mg-cu alloy.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US10/426,561 | 2003-04-29 | ||
| US10/426,561 US6893116B2 (en) | 2003-04-29 | 2003-04-29 | Fluid ejection device with compressive alpha-tantalum layer |
| PCT/US2004/013162 WO2004096555A1 (en) | 2003-04-29 | 2004-04-29 | Fluid ejection device with compressive alpha-tantalum layer |
Publications (2)
| Publication Number | Publication Date |
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| CN1780738A CN1780738A (en) | 2006-05-31 |
| CN1780738B true CN1780738B (en) | 2010-06-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200480011680.1A Expired - Fee Related CN1780738B (en) | 2003-04-29 | 2004-04-29 | Fluid ejection device with compressive alpha-tantalum layer and manufacturing method thereof |
Country Status (6)
| Country | Link |
|---|---|
| US (2) | US6893116B2 (en) |
| EP (1) | EP1618000B1 (en) |
| CN (1) | CN1780738B (en) |
| DE (1) | DE602004026432D1 (en) |
| TW (1) | TWI270410B (en) |
| WO (1) | WO2004096555A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6955835B2 (en) * | 2003-04-30 | 2005-10-18 | Hewlett-Packard Development Company, L.P. | Method for forming compressive alpha-tantalum on substrates and devices including the same |
| US20060063025A1 (en) * | 2004-04-07 | 2006-03-23 | Jing-Yi Huang | Method and system for making thin metal films |
| CN103328220B (en) | 2011-01-31 | 2016-04-27 | 惠普发展公司，有限责任合伙企业 | Fluid ejection assembly and correlation technique |
| JP6041527B2 (en) * | 2012-05-16 | 2016-12-07 | キヤノン株式会社 | Liquid discharge head |
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| US4719477A (en) * | 1986-01-17 | 1988-01-12 | Hewlett-Packard Company | Integrated thermal ink jet printhead and method of manufacture |
| US5221449A (en) * | 1990-10-26 | 1993-06-22 | International Business Machines Corporation | Method of making Alpha-Ta thin films |
| US5279980A (en) * | 1990-02-27 | 1994-01-18 | Fuji Xerox Co., Ltd. | Method of manufacturing a thin-film semiconductor device having an alpha-tantalum first wiring member |
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| DE2215151C3 (en) | 1972-03-28 | 1979-05-23 | Siemens Ag, 1000 Berlin Und 8000 Muenchen | Process for producing thin layers of tantalum |
| WO1992007968A1 (en) * | 1990-10-26 | 1992-05-14 | International Business Machines Corporation | STRUCTURE AND METHOD OF MAKING ALPHA-Ta IN THIN FILMS |
| US5317346A (en) | 1992-03-04 | 1994-05-31 | Hewlett-Packard Company | Compound ink feed slot |
| EP0593372B1 (en) * | 1992-10-14 | 2001-09-19 | Daiki Engineering Co., Ltd. | Highly durable electrodes for eletrolysis and a method for preparation thereof |
| US6162589A (en) | 1998-03-02 | 2000-12-19 | Hewlett-Packard Company | Direct imaging polymer fluid jet orifice |
| US6209991B1 (en) | 1997-03-04 | 2001-04-03 | Hewlett-Packard Company | Transition metal carbide films for applications in ink jet printheads |
| US6139699A (en) | 1997-05-27 | 2000-10-31 | Applied Materials, Inc. | Sputtering methods for depositing stress tunable tantalum and tantalum nitride films |
| US6286939B1 (en) | 1997-09-26 | 2001-09-11 | Hewlett-Packard Company | Method of treating a metal surface to increase polymer adhesion |
| US6013160A (en) * | 1997-11-21 | 2000-01-11 | Xerox Corporation | Method of making a printhead having reduced surface roughness |
| TW520551B (en) | 1998-09-24 | 2003-02-11 | Applied Materials Inc | Method for fabricating ultra-low resistivity tantalum films |
| US6395148B1 (en) | 1998-11-06 | 2002-05-28 | Lexmark International, Inc. | Method for producing desired tantalum phase |
| US6451181B1 (en) | 1999-03-02 | 2002-09-17 | Motorola, Inc. | Method of forming a semiconductor device barrier layer |
| US6265292B1 (en) * | 1999-07-12 | 2001-07-24 | Intel Corporation | Method of fabrication of a novel flash integrated circuit |
| JP3376969B2 (en) * | 1999-09-02 | 2003-02-17 | 株式会社村田製作所 | Surface acoustic wave device and method of manufacturing the same |
| US6387719B1 (en) | 2001-02-28 | 2002-05-14 | Lexmark International, Inc. | Method for improving adhesion |
| US20020158945A1 (en) * | 2001-04-30 | 2002-10-31 | Miller Richard Todd | Heating element of a printhead having resistive layer over conductive layer |
-
2003
- 2003-04-29 US US10/426,561 patent/US6893116B2/en not_active Expired - Fee Related
- 2003-10-28 TW TW092129955A patent/TWI270410B/en not_active IP Right Cessation
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2004
- 2004-04-29 EP EP04750865A patent/EP1618000B1/en not_active Expired - Fee Related
- 2004-04-29 CN CN200480011680.1A patent/CN1780738B/en not_active Expired - Fee Related
- 2004-04-29 WO PCT/US2004/013162 patent/WO2004096555A1/en active Application Filing
- 2004-04-29 DE DE602004026432T patent/DE602004026432D1/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4719477A (en) * | 1986-01-17 | 1988-01-12 | Hewlett-Packard Company | Integrated thermal ink jet printhead and method of manufacture |
| US5279980A (en) * | 1990-02-27 | 1994-01-18 | Fuji Xerox Co., Ltd. | Method of manufacturing a thin-film semiconductor device having an alpha-tantalum first wiring member |
| US5221449A (en) * | 1990-10-26 | 1993-06-22 | International Business Machines Corporation | Method of making Alpha-Ta thin films |
Also Published As
| Publication number | Publication date |
|---|---|
| US20050175768A1 (en) | 2005-08-11 |
| CN1780738A (en) | 2006-05-31 |
| WO2004096555A1 (en) | 2004-11-11 |
| EP1618000A1 (en) | 2006-01-25 |
| US7132132B2 (en) | 2006-11-07 |
| US6893116B2 (en) | 2005-05-17 |
| TWI270410B (en) | 2007-01-11 |
| US20050083378A1 (en) | 2005-04-21 |
| DE602004026432D1 (en) | 2010-05-20 |
| TW200422104A (en) | 2004-11-01 |
| EP1618000B1 (en) | 2010-04-07 |
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